CN104769390B - With the method and apparatus of X-ray measurement film thickness - Google Patents
With the method and apparatus of X-ray measurement film thickness Download PDFInfo
- Publication number
- CN104769390B CN104769390B CN201380055724.XA CN201380055724A CN104769390B CN 104769390 B CN104769390 B CN 104769390B CN 201380055724 A CN201380055724 A CN 201380055724A CN 104769390 B CN104769390 B CN 104769390B
- Authority
- CN
- China
- Prior art keywords
- basalis
- film layer
- thickness
- ray
- intensity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B15/00—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons
- G01B15/02—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons for measuring thickness
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20066—Measuring inelastic scatter of gamma rays, e.g. Compton effect
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/063—Investigating materials by wave or particle radiation by diffraction, scatter or reflection inelastic scatter, e.g. Compton effect
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Electromagnetism (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Length-Measuring Devices Using Wave Or Particle Radiation (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The present invention relates to the method and apparatus for the thickness using X-ray measurement film layer.According to the present invention, calibration curve be by comparing by being determined included in the difference and the thickness of film layer that are formed with basalis and thereon between the intensity of the signal scattered by the special elementses in the basalis of the reference sample of the basalis of film layer, and pass through the difference of intensity between the signal that the element-specific being contained in the basalis with the target sample with the basalis for being formed with film layer thereon in the reference sample with basalis is scattered and calibration curve be compared thus determine target sample film layer thickness.
Description
Technical field
The method and the equipment using methods described of the thickness of film are measured the present invention relates to use x-ray, and it is more true
Say with cutting and be directed to use with being configured to using special included in the basalis and/or film layer of reference sample and target sample
The method and its equipment of the thickness of the x-ray measurement film layer of component, and further more particularly to using x-ray measure thin
Method and equipment using methods described of the nano-level thin-membrane thickness without destroying target sample.
Background technology
This part provides the background information that is not necessarily prior art relevant with the present invention.
Film thickness is routinely by respectively using SEM (SEM), FESEM (Flied emission scanning electrons
Microscope), STEM (scanning transmission electron microscope), vortex flow method for sensing, ultrasonic method and using X-ray high-energy
Sensitive method or and combination with one another.Among these methods, the method for X-ray is used to cause x-ray bombardment to destination object,
For example, film or the film formed by metallic film and/or polymer are used with the intensity in response to the signal obtained therefrom
Non-contact method measures thickness.Measured film thickness method using X-ray can use single object as target or just
Target is used as in the object of production.
For example, the thickness of destination object (for example, metallic film or film) can be measured while having predetermined in real time
The destination object of thickness is manufactured by one of rolling methods, the method for manufacturing objective object, and can be by adjusting
Save the product that the thickness of destination object manufactures good quality with constant flat thickness.
The amount that the quantum x-ray of destination object can be permitted the pass through using the non-contact thickness measuring device of X-ray is led to
Cross detector to be detected, or penetrate the fluorescent X-ray of destination object and measure detection to measure the thickness of destination object.
The amount of the quantum x-ray detected in response to the material of destination object by detector or the amount of fluorescent X-ray are in absorption coefficient, close
Change on degree and thickness, wherein to be irradiated to X-ray target and from X-ray objective emission without destination object
The amount of quantum x-ray and irradiation are with the amount of the X-ray through destination object through destination object and from X-ray objective emission
Carry out relatively, the thickness of destination object can be learnt by the relative different of inspection therebetween whereby.
However, by using X-ray when targets are present with the difference for the quantum amount launched when destination object is not present
Measure that the method for the thickness of destination object is subjected to disadvantage is that understanding the amount of quantum when destination object is not present
The basic premise of difference, making it difficult to apply the method and independently formed to measure in the thickness on substrate or basalis or be difficult to apply
Plus the method is to continuous process.Exactly, even if sensitive X-ray method is used for high-energy, and if film thickness
In some nanometers (nm) below, then be also difficult to the film thickness for measuring nanometer level.
Accordingly, it would be desirable to solve disadvantages mentioned above.
The content of the invention
This part provides the overall outline to the present invention, and is not the comprehensive of its full breadth or its all feature
Disclosure.
Accordingly, it would be desirable to can be used for the simple structure of the film of some nanometers of thickness measured film thickness equipment and
Measured film thickness method, and therefore it is an object of the present invention to accurately measure some nanometers thickness film without destruction
Target sample.
In addition, the present invention is provided to measure the method and its equipment of film thickness, methods described is configured to simply
And the thickness of film is easily only measured, method is directly by with the film layer being formed on substrate or the target pair of basalis
As object and available for unit process and continuous processing.
However, it should be emphasized that the invention is not restricted to specific disclosure, as explained above.It should be understood that art
Technical staff be appreciated that other technological subjects not mentioned herein.
There is provided the method for the thickness for measuring film using x-ray, the side in the general aspect of the present invention
Method includes：
The intensity of the signal scattered by the particular components included in basalis is detected, method is to be irradiated to x-ray
The basalis of reference sample；
The intensity of the signal scattered by the particular components included in basalis is detected, method is to be irradiated to x-ray
It is formed at the film layer on the basalis of reference sample；
Calibration curve is determined, method is to compare the letter correspondingly detected from basalis irradiating step and film layer irradiating step
The thickness of difference and film layer between number intensity；
The intensity of the signal scattered by the particular components included in basalis is detected, method is to be irradiated to x-ray
It is formed at the film layer on the basalis of target sample；And
The thickness of the film layer of target sample is determined, method is compared correspondingly in basalis irradiating step and target sample
Difference between the intensity and calibration curve of the signal detected in irradiating step.
Preferably, but nonessential, basalis can be glass substrate.
Preferably, it is but nonessential, the thickness of film layer can in the range of 10~400nm, and can be by
Metal level selected from the group being made up of silver, copper, nickel, manganese, chromium, iron and gold.
Preferably, but nonessential, particular components can be selected from the group being made up of C, H, O, Ca, Na, Si and Ag.
Preferably, but nonessential, particular components can be not present in film layer, but can be only present in substrate
In layer.
Preferably, but nonessential, x-ray can be irradiated by Portable X RF (XRF) spectrometer.
Preferably, but nonessential, methods described may further include is formed at ginseng using electron microscope measurement
Examine the thickness of the film on the basalis of sample.
Preferably, but nonessential, calibration curve can be determined by below equation：
[equation 1]
I/Io=exp [- (μ/ρ) X]
I：Relative to the intensity of the return signal of film layer
Io：Relative to the intensity of the return signal of basalis
μ：The attenuation coefficient of film layer
ρ：The density of film layer
X：The thickness of film layer
Preferably, but nonessential, the step of determining calibration curve can be included between the intensity by comparison signal
Difference and the thickness of film layer be corrected.
It is described to set there is provided the equipment of the thickness for measuring film using x-ray in another general aspect of the present invention
It is standby to include：
X-ray generator, x-ray is irradiated to the film of reference sample, the basalis of target sample or target sample by it
Layer；
Detector, it detects the intensity of the signal scattered from reference sample or target sample；And
Controller, it is by comparing by included in basalis and with the ginseng of the basalis formed by film layer
The thickness of difference and film layer between the intensity for the signal for examining the particular components scattering in the basalis of sample determines that calibration is bent
Line, and by compare by included in the basalis of the target sample with the basalis formed by film layer with
The difference of the intensity of the signal of particular components scattering in the reference sample of basalis determines the thin of target sample with calibration curve
The thickness of film layer.
The apparatus and method for the thickness for being used to measure film using x-ray according to the exemplary embodiment of the present invention have
The effect of profit, is the thickness that can accurately measure nano-level thin-membrane without destruction target sample, by determining target sample
The thickness of this film, by comparing by the reference sample included in the basalis formed with basalis and by film layer
The thickness of difference and film layer between the intensity of the signal of particular components scattering in basalis determines calibration curve, and leads to
Cross compare by included in the basalis of the target sample with the basalis formed by film layer with basalis
The difference of the intensity of the signal of particular components scattering in reference sample determines the thickness of the film layer of target sample with calibration curve
Degree.
In addition, the present invention can provide for using x-ray measure film thickness method and apparatus, methods described and
Equipment be configured to use the test acceptor with the film layer being formed on substrate or basalis as object easily and
The thickness of film layer is simply measured, and is configured to be equally used in unit process and continuous process.
Brief description of the drawings
In order to illustrate the principle of the present invention, hereinafter report that to be related to its excellent for diagram, the purpose of example and description
Select some accompanying drawings of embodiment, although they are not intended to be in detail.Accompanying drawing is according to concept of the present invention only by means of example
Not one or more exemplary embodiments are depicted by means of limitation.In the accompanying drawings, identical reference number refer to it is identical or
Similar element.
Therefore, by the described in detail below of some exemplary embodiments, it will be better understood with reference to exemplary drawings many
Potential actual and useful embodiment is planted, in the accompanying drawings：
Fig. 1 is concept map of the diagram according to the x-ray scatter state on the base layer of the exemplary embodiment of the present invention；
Fig. 2 is curve map of the diagram according to an example of the calibration curve of the present invention；
Fig. 3 to 14 is to be shot according to the exemplary embodiment of the present invention by the FEM SEM of the sample 1~12 with silver layer
The photo correspondingly analyzed；
Figure 15 is thickness measurement of the diagram according to the sample #10 of the use x-ray of the exemplary embodiment of the present invention
Display screen；
Figure 16 and 17 is the FEM SEM for passing through sample #13~14 with layers of copper according to the exemplary embodiment of the present invention
The photo correspondingly analyzed shot；And
Figure 18 and 19 is to be passed through according to the exemplary embodiment of the present invention with silver layer and the sample of layers of copper 15~16
The photo correspondingly analyzed that FEMSEM is shot.
Embodiment
Disclosed embodiment and its advantage are best understood by by reference to Fig. 1-19 of accompanying drawing, identical label is used for each accompanying drawing
Identical and corresponding part.For one of ordinary skill in the art after refering to the following drawings and its detailed description
For disclosed embodiment further feature and advantage will be apparent or will become obvious.Desirably it is all this
Class additional features and advantage are included in the range of disclosed embodiment, and are protected by accompanying drawing.In addition, illustrated accompanying drawing is only
Only it is exemplary and is not intended to confirm or implies any of the environment that can implement on not be the same as Example, framework or process
Limitation.Therefore, described aspect be intended to cover all such changes for belonging to the scope of the present invention and novel idea, modification and
Change.
Meanwhile, term used herein is the purpose merely for description particular and is not intended to limit this hair
It is bright.Term " first " herein, " second " etc. simultaneously refer not to any order, quantity or importance, and are practically used for distinguishing
One element and another element.For example, the second element without departing from the scope and spirit in the present invention
The first element can be denoted as, and similarly, the first element can be denoted as the second element.
As used herein, term " one " and " one " are not offered as the limitation of quantity herein, but actually
Represent the presence of at least one reference items.As used herein, singulative " one ", " one " and " described " intention
Plural form is equally included, unless the context clearly indicates otherwise.
Will be further understood that, term " comprising " or "comprising" specified when in for this specification institute's features set forth, region,
Entirety, step, operation, the presence of element and/or component, but it is not excluded that one or more of the other feature, region, entirety,
Step, operation, element, component and/or the presence of its group or addition.
In addition, " exemplary " is intended merely to mean an example and not the best.In addition, it will also be understood that being retouched herein
Feature, layer and/or the element painted are in order at simple and understandable purpose and said relative to each other with specific dimensions and/or orientation
It is bright, and actual size and/or orientation may be substantially different from it is illustrated.
That is, for the sake of clarity the size and relative size of layer, region and/or other elements can be with the accompanying drawings
Zoom in or out.Identical label refers to identical element and will omit the explanation repeated each other in the text.As can be with
It is used in the present context, term " substantially " and " approximate " provide the row of the correlation between its corresponding term and/or project
The tolerance limit that industry receives.
For reference purposes, the thickness of film thickness and film can be interchangeably used for the present invention.
Hereinafter, it will be described in detail by referring to the drawings according to the present invention for the thickness using x-ray measurement film
Method and the equipment using methods described.
The method of thickness for measuring film using x-ray is arranged such that x-ray is correspondingly irradiated to by thin
The reference sample of the basalis of film layer formation and target sample is irradiated to, and the thickness of the film of target sample is using logical
The difference measurement of the intensity of the signal for the particular components scattering crossed included in basalis.
That is, calibration curve is first by using in response to as the ginseng with the basalis formed by film layer
Examine the thickness for the film layer that the object of sample is used change be included in particular components scattering in basalis signal intensity
Difference determine, be compared by calibration curve, method is to determine as with the mesh of basalis formed by film layer
The intensity of the signal of the particular components scattering of the object of standard specimen sheet, and determine the thickness of film layer.
Now, film layer can be organic film or inorganic thin film, and can preferably by selected from by silver, copper, nickel,
The metal for the group that manganese, chromium, iron and gold are constituted is formed.
As the present inventor check as a result, it is difficult to measure the thickness of the metal level formed by titanium or molybdenum.In addition, film layer
In the range of 10~400nm, preferably in the range of 50~300nm, and if film layer deviates the scope, then
Because calibration curve is not straight in proportion by electron emission coefficiency, so being difficult with x-ray measurement thickness.
In addition, basalis is the substrate formed by film layer, and it can be variable substrate as known in the art
One or the layer that is stacked by one or more film layers.It is a feature of the present invention that using by included in basalis or being present in thin
The intensity of the signal of particular components scattering in other film layers below film layer, wherein basalis preferably includes one or many
Individual particular components.
For this purpose, the step of present invention is by comprising following item is performed successively：Basalis irradiating step, film irradiation step
Suddenly, calibration curve determines that step, target sample irradiating step and thin film layer thickness determine step.
First, basalis irradiating step is to be irradiated to the basalis of reference sample to detect by included in base by x-ray
The intensity of the signal of particular components scattering in bottom.That is, x-ray is irradiated to the reference sample without film layer
Basalis to detect the intensity of signal, and signal intensity later with the intensity of the signal of reference sample formed by film layer
It is compared to determine to change by film layer the intensity of the signal of (reduction).
X-ray is irradiated to organic film reference sample or organic film target sample, and wherein x-ray can be sent out by x-ray
Raw device or the generation of radioisotopic target material.
X-ray irradiating step can include two methods, one be using the method for x-ray generator and another be
Use radioisotopic method.
X-ray generator generates x-ray, and method is to allow to occur by the particles collision x-ray that photon and electronics accelerate
Target material inside device, the step of as generating special x-ray, and works as generated x-ray and passes through apparatus surface
Window when only launch for the special x-ray in the inside of target material.Therefore, from the target material inside x-ray generator or
The special x-ray generated in radio isotope passes through the collision with organic thin film layer reference sample or organic film target sample
And scatter.
In this process, due to being present in organic thin film layer reference sample or organic film target as analysis of material
C, H and O element in sample, special x-ray generates non-resilient Compton scattering.For example, the basalis of reference sample or
The target sample formed by glass substrate can be included such as Ca and particular components receiving wherein, and scattered by specific group
The intensity for the signal penetrated can be detected by portable x-ray fluorescence (XRF) spectrometer.
Portable X RF spectrometers are routinely used for the content for the particular components that measurement is included in film layer, but this hair
It is bright to be characteristically used for the thickness of the ionization meter film using the signal in response to particular components using XRF spectrometers.Therefore,
Any material selected from the group being made up of C, H, O, Ca, Na, Si and Ag can be included according to particular components of the present invention
Material or more material.However, consider that particular components are preferably a kind of component for accuracy, and particular components are more preferably
It is not present in film layer, but exists only in basalis.
The intensity of the signal of the x-ray of scattering or non-resilient Compton scattering line with by organic thin film layer reference sample or
The incidence angle (θ 1) of x-ray incidence on organic film target sample changes and the angle (output angle θ 2) to scatter therefrom
Change, analytical performance (for example, detectable limit) can be in response to organic thin film layer reference sample or organic film target sample whereby
This device situation is strengthened by the determination of best angle.
The intensity of scattered signal can by after collision by with organic thin film layer reference sample or organic film mesh
The special x-ray or Compton inelastic scattering x-ray of standard specimen sheet or the Compton scattering signal generation only in fluorescent x rays
The selection of Rayleigh elastic scattering x-ray is detected.Can be by using solid corresponding to the x-ray wavelength of Compton scattering signal
State crystal diffraction, and special peak signal can use the detector being arranged at special angle to be obtained by Compton scattering
Selective enumeration method.In response to analysis of the Compton scattering by using the region of peak value, angular instrument can be installed to detect
The Compton scattering signal of preset range.
Next, thin films scattering step is that the intensity of scattered signal is detected by the particular components included in basalis,
Method is that x-ray is irradiated to the film layer being formed on the basalis of upper reference sample.That is, although basalis irradiates
Step has detected the intensity of signal relative to the reference sample without film layer, but film layer irradiating step will detect have
There is the intensity of the signal of the reference sample of film layer, and the intensity of two kinds of signals is compared to determine to change by film layer
Become the intensity of the signal of (reduction).
Fig. 1 is diagram according to the general of the wherein x-ray scatter state on the base layer of the exemplary embodiment of the present invention
Read figure, wherein in the case of x-ray is radiated on the basalis formed by film layer, the signal scattered by film layer it is strong
It is to change to spend compared to the basalis without film layer is formed as.That is, the number of the launching electronics of the x-ray of scattering
Mesh can be reduced by film layer, and the signal of x-ray can reduce, or wavelength can change, this thickness in response to film layer
Degree is presented differently from, and this is proportional to the thickness of film layer.
Therefore, calibration curve determines step by by comparing by basalis irradiating step and the actual thickness with film layer
The difference of the intensity for the signal that the film layer irradiating step of degree is correspondingly detected determines calibration curve.That is, with base
In the reference sample of bottom and reference sample with the basalis formed by film layer, calibration curve passes through in response to film
The change for the particular components that the actual (real) thickness of layer is contained in basalis reduces the difference for using the signal intensity as substrate
Determined.
It is desirable for this purpose that understanding the actual (real) thickness of film layer in advance so that the method according to the invention can be further
The thickness for the film layer being formed at including the use of electron microscope measurement on the basalis of reference sample.
Fig. 2 is curve map of the diagram according to an example of the calibration curve of the present invention, wherein, y-axis is defined on basalis
The difference of the intensity of the signal correspondingly detected in irradiating step and film layer irradiating step, x-axis is defined in response to intensity
Difference is by the thickness of the SEM film layers measured, and the reference sample for wherein using the silver layer in glass substrate to be formed is made
For object, the intensity of the signal based on the calcium constituent scattering included in glass substrate.
The determination of calibration curve can pass through x-ray mass attentuation coefficient：(μ/p) is determined, is such as shown in equation 1 below
Go out.That is, film layer is relative to reference sample or the ratio and film layer of the intensity of the signal of the basalis of target sample
Density it is proportional, be inversely proportional to the thickness, and the attenuation coefficient (μ) of film layer can pass through the type of film layer, composition, thickness
The incidence angle of degree and x-ray is arranged differently than.
[equation 1]
I/Io=exp [- (μ/ρ) X]
I：Relative to the intensity of the return signal of film layer
Io：Relative to the intensity of the return signal of basalis
μ：The attenuation coefficient of film layer
ρ：The density of film layer
X：The thickness of film layer
Above-mentioned equation 1 can be μ/ρ=X-1In(Io/ I), and if film layer is sandwich construction [t], then multilayer knot
The thickness of structure can be calculated by I.e.X=ρ t.
In addition, calibration curve determines that step can be included by between the intensity of comparison signal and the actual (real) thickness of film layer
Difference correction, to improve accuracy.
Unceasingly, target sample irradiating step may be embodied in the film layer being formed on the basalis of target sample and can photograph well
X-ray is penetrated to detect the intensity of the signal scattered by the particular components being contained in basalis.
Although above-mentioned steps determine calibration curve, target sample irradiating step using reference sample as object
Using relative to the intensity of the return signal of the target sample detection x-ray as analysis object.Target sample is unbroken, but
Be x-ray direct irradiation on the basalis containing film layer, the basalis and film layer of wherein target sample are preferably phase
With or similar to reference sample those for being compared with reference sample.
In addition, film layer determines step by comparing correspondingly in basalis irradiating step and target sample irradiating step
The difference of the intensity of the signal detected determines the thickness of the film layer of target sample.That is, calculating correspondingly in substrate
The difference of the intensity of signal being detected in layer irradiating step relative to reference sample and being detected in target sample irradiating step
It is different without destruction target sample, the thickness of the film layer to determine target sample indirectly is then compared with calibration curve.
There is provided the equipment of the thickness for measuring film using x-ray in another general aspect of the present invention, wherein
Specifically the equipment includes x-ray generator, detector and controller.
X-ray is irradiated to the basalis or film layer of reference sample or target sample by x-ray generator.X-ray occurs
Device includes x-ray tube (not shown), high pressure generator (not shown) and various safety circuits (not shown).It is used as the pole of thermoelectron 2
The x-ray tube of vacuum tube accelerates the thermoelectron from negative electrode (being typically tungsten filament) and acceleration thermoelectron is collided with anode to produce
Raw x-ray.Typically widely disperse towards the electron stream of anode so that appropriate magnetic field is applied into Wehnelt cylinder, whereby
Prevent electron stream from deviateing.In order to generate x-ray, high pressure generator generates negative high voltage and the negative high voltage is fed into x
Ray tube.During the generation of x-ray high capacity of the safety circuit warning x-ray generator at x-ray generator, high pressure and
The appearance of low pressure.
Detector is used for the intensity for detecting the signal scattered from reference sample or target sample.Detector is received from referring to sample
X-ray that this and target sample reflect is to detect the strength level of the x-ray of reflection.That is, detectors measure is from sample
The intensity level of the x-ray of substrate reflection.Detector can be disposed in pairs, and an example of detector can be PC (ratios
Counter) and SC (scintillation counter).
The present invention can further comprising be placed in from sample substrates reflect x-ray path on Analyze ＆ separate device with
Special x-ray of the filtering with specific wavelength in the x-ray reflected from sample substrates.Now, reflected from sample substrates
X-ray correspond to the x-ray that is generated when electronics is moved to low-lying level while being irradiated in sample substrates from high level.
By the thickness of film layer, controller is included in what is correspondingly had basalis and formed by film layer by comparing
The difference of the content of particular components in the basalis of the reference sample of basalis determines calibration curve；And it is bent by calibrating
Line, is included in the basalis of the target sample with the basalis formed by film layer and the ginseng with basalis by comparing
Examine the content of the particular components in sample difference determine target sample film layer thickness.
The present invention can use x-ray accurately to measure thin nano-level thin-membrane thickness without destroying target sample.In addition, this
Invention can provide the method and apparatus of the thickness for measuring film using x-ray, methods described and equipment be configured so that
Easily and film is simply measured with the test acceptor with the film layer being formed on the substrate or basalis as object
The thickness of layer, and be configured to be equally used in unit process and continuous process.
The present invention can be more fully understood by following exemplary embodiment, the exemplary embodiment is only by means of example
There is provided, and not by means of limitation.
First exemplary embodiment：The measurement of silver thickness
The present inventor prepares sample #1~12 each with silver layer, X-ray used according to the invention on a glass substrate
The thickness of silver layer is measured with FEM SEM, and obtains the following result as shown in table 1 and Fig. 3 to 14.Fig. 3 to 14 is basis
The photo correspondingly analyzed that the exemplary embodiment of the present invention is shot by the FEM SEM of the sample 1~12 with silver layer；
【Table 1】
As proved in table 1, it may be noted that according to the present invention is in the analysis result by FEM SEM and passes through X-ray
There is very big or close similitude between analysis result.
Figure 15 is thickness measurement of the diagram according to the sample #10 of the use x-ray of the exemplary embodiment of the present invention
Display screen.
Second exemplary embodiment：The measurement of copper layer thickness
The present inventor prepare on a glass substrate the sample #13 and 14 with layers of copper, X-ray used according to the invention and
FEM SEM measure the thickness of layers of copper, and obtain the following result as shown in table 2 and Figure 16 and 17.
Figure 16 and 17 is the FEM SEM for passing through sample #13~14 with layers of copper according to the exemplary embodiment of the present invention
The photo correspondingly analyzed shot.
【Table 2】
| Sample number | 13 | 14 |
| Pass through FEM SEM analysis result [nm] | 44 | 70 |
| Pass through the analysis result [nm] of X-ray | 43 | 69 |
As proved in table 2, it may be noted that according to the present invention is in the analysis result by FEM SEM and passes through X-ray
There is very big or close similitude between analysis result.
3rd exemplary embodiment：The measurement of silver thickness and copper layer thickness
The present inventor prepares on a glass substrate to be penetrated with layers of copper and the sample #15 of silver layer and 16, X used according to the invention
Line and STEM (scanning transmission electron microscope) method measure the thickness of layers of copper.
1. transmission detector (STEM) is arranged on to analyze the sample manufactured with film layer (thin slice) shape on STEM, wherein
Analyze data shape is identical with above-mentioned FE SEM methods, but the preprocess method of sample is different.
2. when preparing sample, FIB (focused ion beam) method be used for FEM SEM situation, and FIB it is adjusted with point
The formation in the section of sample is analysed, and the sample of chip shape is fabricated to the manufacturer of its manufacture method and transmission electron microscope
Method is identical.
3. sample is the chip shape being horizontally fixed on electron microscope, and is irradiated to obtain with electron beam
Image is obtained, wherein the thickness of the film coated is the software tape measure using accurate calibration.Its result in table 3 below and
Shown in Figure 18 and 19.
Figure 18 and 19 is to pass through sample #15~16 with silver layer and layers of copper according to the exemplary embodiment of the present invention
The photo correspondingly analyzed that FEM SEM are shot.
【Table 3】
As proved in table 3, it may be noted that according to the present invention is in the analysis result by FEM SEM and passes through X-ray
There is very big or close similitude between analysis result.
4th exemplary embodiment：The measurement of the thickness of metal level
The present inventor prepares silver, copper, nickel and the iron sample of each thickness with 500nm on a glass substrate, and makes
Each thickness is measured with FEM SEM.Each thickness of metal level is to use to be measured according to the x-ray method of the present invention, and
It the results are provided in table 4 below.
【Table 4】
| Metal | Silver | Copper | Nickel | Iron |
| Pass through the analysis result of X-ray | Thickness immeasurability | Thickness immeasurability | Thickness immeasurability | Thickness immeasurability |
As proved in table 4, it may be noted that can not use has approximate 500nm according to the x-ray method measurement of the present invention
The thickness of the metal level of level or bigger.
Although describing the present invention by reference to its multiple illustrative examples, it should be understood that the technology people of art
Member can be designed that many other modifications and embodiment in the spirit and scope of the principle by the present invention is belonged to.
More specifically, it is understood that there may be the theme combination belonged in the present invention, accompanying drawing and the scope of the appended claims
The part of configuration and/or the variations and modifications of arrangement.Except changing and modifications it in part and/or arrangement
Outside, alternative use also will be apparent for those skilled in the art.
Claims (11)
1. a kind of method for being used to be measured the thickness of film using x-ray, methods described is included：
The intensity of the signal scattered by the particular components included in basalis is detected, method is that x-ray is irradiated into reference
The basalis of sample；
The intensity of the signal scattered by the particular components included in the basalis is detected, method is to be irradiated to x-ray
It is formed at the film layer on the basalis of the reference sample；
Calibration curve is determined, method is that the signal compared correspondingly from basalis irradiating step and the detection of film layer irradiating step is strong
The thickness of difference and the film layer between degree；
The intensity of the signal scattered by the particular components included in basalis is detected, method is to be irradiated to x-ray to be formed
Film layer on the basalis of target sample；And
Determine the thickness of the film layer of the target sample, method be compare correspondingly in the basalis irradiating step and
Difference between the intensity and the calibration curve of the signal detected in the target sample irradiating step,
Characterized in that, in the calibration curve, y-axis is defined as the phase in basalis irradiating step and film layer irradiating step
The difference of the intensity of the signal detected with answering, x-axis is defined as the actual (real) thickness of the film layer measured by electron microscope；Institute
The thickness of film layer is stated in the range of 50-300nm；And the calibration curve passes through electron emission coefficiency Cheng Zhi in proportion
Line.
2. according to the method described in claim 1, wherein the basalis is glass substrate.
3. according to the method described in claim 1, wherein the film layer be include by selected from by silver, copper, nickel, manganese, chromium, iron and
The metal level of at least one in the group of gold composition.
4. according to the method described in claim 1, the particular components, which are included, is selected from what is be made up of C, H, O, Ca, Na, Si and Ag
At least one in group.
5. according to the method described in claim 1, wherein the particular components are one in C, H, O, Ca, Na, Si and Ag.
6. according to the method described in claim 1, wherein the particular components are not present in film layer, but exist only in institute
State in basalis.
7. according to the method described in claim 1, wherein x-ray is irradiated by Portable X RF (XRF) spectrometer.
Using electricity before 8. according to the method described in claim 1, it further comprises the step of the determination calibration curve
Son is measured microscopically the thickness for the film being formed on the basalis of the reference sample.
9. the method according to any claim in claim 1 to 8, wherein the calibration curve passes through equation 1 below
It is determined that：
[equation 1]
I/Io=exp [- (μ/ρ) X], wherein,
I：Relative to the intensity of the return signal of film layer
Io：Relative to the intensity of the return signal of basalis
μ：The attenuation coefficient of film layer
ρ：The density of film layer
X：The thickness of film layer.
10. the method according to any claim in claim 1 to 8, wherein the step of determining the calibration curve is wrapped
It is corrected containing the difference and the thickness of film layer between the intensity by comparison signal.
11. a kind of equipment for being used to be measured the thickness of film using x-ray, the equipment is included：
X-ray generator, x-ray is irradiated to the film of reference sample, the basalis of target sample and the target sample by it
Layer；
Detector, it detects the intensity of the signal scattered from the reference sample and the target sample；And controller, it leads to
Cross and compare by included in the basalis of the reference sample with basalis and with the basalis formed by film layer
The thickness of difference and the film layer between the intensity of the signal of particular components scattering determines calibration curve, and by comparing
By included in the basalis of the target sample with the basalis formed by the film layer with institute
The difference for stating the intensity of the signal of the scattering of the particular components in the reference sample of basalis determines institute with the calibration curve
State the thickness of the film layer of target sample, it is characterised in that the y-axis of the calibration curve be defined as in basalis irradiating step and
The difference of the intensity of the signal correspondingly detected in film layer irradiating step, x-axis is defined as what is measured by electron microscope
The thickness of film layer；The thickness of the film layer is in the range of 50-300nm；And the calibration curve passes through electron emission
Coefficient is in line in proportion.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020120119379 | 2012-10-26 | ||
| KR1020120119379A KR101241007B1 (en) | 2012-10-26 | 2012-10-26 | Method and apparatus for measuring thickness of thin film using x-ray |
| PCT/KR2013/001312 WO2014065473A1 (en) | 2012-10-26 | 2013-02-20 | Method and device for measuring thickness of thin film layer using x-rays |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104769390A CN104769390A (en) | 2015-07-08 |
| CN104769390B true CN104769390B (en) | 2017-09-29 |
Family
ID=48181382
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201380055724.XA Active CN104769390B (en) | 2012-10-26 | 2013-02-20 | With the method and apparatus of X-ray measurement film thickness |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US9644956B2 (en) |
| JP (1) | JP6167182B2 (en) |
| KR (1) | KR101241007B1 (en) |
| CN (1) | CN104769390B (en) |
| DE (1) | DE112013005159T5 (en) |
| WO (1) | WO2014065473A1 (en) |
Families Citing this family (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101568489B1 (en) | 2013-12-12 | 2015-11-11 | 주식회사 포스코 | Apparatus for measuring thickness and component content of coating layer |
| US9594035B2 (en) | 2014-04-25 | 2017-03-14 | Revera, Incorporated | Silicon germanium thickness and composition determination using combined XPS and XRF technologies |
| KR101510592B1 (en) | 2014-04-25 | 2015-04-09 | 주식회사 포스코 | Method for measuring thickness of coating layer |
| KR102527483B1 (en) * | 2014-06-24 | 2023-04-28 | 리베라 인코퍼레이티드 | Feed-forward of multi-layer and multi-process information using xps and xrf technologies |
| US9651369B1 (en) * | 2015-03-27 | 2017-05-16 | Neocera, Llc | Method and system for in-situ determination of a chemical composition of films during growth process |
| EP3124912B1 (en) * | 2015-07-30 | 2019-01-16 | Unity Semiconductor GmbH | Method and assembly for determining the thickness of a layer in a stack of layers |
| CN105157629A (en) * | 2015-09-18 | 2015-12-16 | 深圳市和胜金属技术有限公司 | Method for measuring thickness of vanadium carbide thin film based on X-ray spectrometer |
| CN105466368A (en) * | 2016-01-01 | 2016-04-06 | 广州兴森快捷电路科技有限公司 | Nickel base surface treatment weldability analysis method |
| KR101716860B1 (en) | 2016-05-30 | 2017-03-27 | 주식회사 아이에스피 | A X-ray fluorescence spectrometer |
| KR101948416B1 (en) | 2017-03-17 | 2019-04-29 | 한양대학교 에리카산학협력단 | Device for measuring density of film layer and method for measuring density of film layer using same |
| WO2018229848A1 (en) * | 2017-06-13 | 2018-12-20 | 株式会社日立ハイテクノロジーズ | Charged particle beam device and method for measuring thickness of sample |
| CN108508052B (en) * | 2018-06-11 | 2023-10-20 | 西北核技术研究所 | X-ray fluorescence thin layer quality thickness measurement system and method based on reference element |
| JP6618059B1 (en) * | 2018-07-09 | 2019-12-11 | 株式会社リガク | X-ray analysis system, X-ray analysis apparatus and vapor phase decomposition apparatus |
| JP7483742B2 (en) * | 2019-03-12 | 2024-05-15 | ノヴァ メジャリング インスツルメンツ インコーポレイテッド | Method and system for monitoring a deposition process - Patents.com |
| CN110017798A (en) * | 2019-04-04 | 2019-07-16 | 浙江上方电子装备有限公司 | A kind of method and device detecting film thickness |
| CN110296670A (en) * | 2019-07-23 | 2019-10-01 | 钛科优控(江苏)工业科技有限公司 | A kind of high-precision laser ray synchro measure all-in-one machine |
| CN112697080A (en) * | 2020-12-16 | 2021-04-23 | 长江存储科技有限责任公司 | Method for measuring thickness of thin film layer |
| KR102434597B1 (en) | 2021-02-05 | 2022-08-23 | 주식회사 아이에스피 | system and method for measuring the thickness of continuous prints based on X-ray fluorescence analysis |
| CN113008171A (en) * | 2021-03-19 | 2021-06-22 | 长江存储科技有限责任公司 | Method for determining thickness of sample |
Family Cites Families (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52125352A (en) * | 1976-04-13 | 1977-10-21 | Seiko Instr & Electronics Ltd | Standard sample vessel for measuring thickness of coatings |
| JPS6385309A (en) * | 1986-09-30 | 1988-04-15 | Kawasaki Steel Corp | Method and apparatus for measuring thickness of liquid film on plate-like material |
| JPH0619268B2 (en) * | 1987-08-07 | 1994-03-16 | 日本鋼管株式会社 | Method for measuring thickness of coating film on metal |
| JPS6441510A (en) | 1987-08-08 | 1989-02-13 | Mitsubishi Electric Corp | Current/voltage converting circuit |
| JP2861598B2 (en) * | 1992-03-02 | 1999-02-24 | 日本鋼管株式会社 | Method and apparatus for measuring coating thickness on metal and method and apparatus for producing coated metal body |
| US5195117A (en) * | 1992-04-24 | 1993-03-16 | University Of Houston | Method for using secondary radiation scattering to evaluate the thickness of materials |
| JP3373698B2 (en) * | 1995-06-12 | 2003-02-04 | 理学電機工業株式会社 | X-ray analysis method and X-ray analyzer |
| JPH08334481A (en) * | 1996-07-25 | 1996-12-17 | Shimadzu Corp | X-ray fluorescent analysis |
| JPH10221047A (en) | 1997-02-03 | 1998-08-21 | Jeol Ltd | Fluorescent x-ray film thickness analyzer and method |
| US6111929A (en) * | 1997-03-14 | 2000-08-29 | Xrf Corporation | Scanning X-ray fluorescence analyzer |
| US6399944B1 (en) * | 1999-07-09 | 2002-06-04 | Fei Company | Measurement of film thickness by inelastic electron scattering |
| US20020190207A1 (en) * | 2000-09-20 | 2002-12-19 | Ady Levy | Methods and systems for determining a characteristic of micro defects on a specimen |
| JP2002213935A (en) | 2001-01-15 | 2002-07-31 | Murata Mfg Co Ltd | Method of measuring film thickness |
| KR20040072780A (en) * | 2003-02-11 | 2004-08-19 | 삼성전자주식회사 | Method for measuring a thickness of a thin layer |
| KR100721810B1 (en) * | 2005-07-19 | 2007-05-25 | 포항공과대학교 산학협력단 | Method for fourier analysis of x-ray reflectivity of ultra thin layer thickness measurement |
| CN101133300B (en) * | 2005-09-26 | 2010-09-08 | 杰富意钢铁株式会社 | Method for measuring surface layer oxide film thickness of galvanized steel plate |
| CN1316229C (en) * | 2005-09-30 | 2007-05-16 | 电子科技大学 | Thin-membrane thickness and density measurement without sampler |
| CN101319886A (en) * | 2008-04-21 | 2008-12-10 | 北大方正集团有限公司 | Method for measuring film thickness of silicon substrate thin film |
| JP2010014432A (en) * | 2008-07-01 | 2010-01-21 | Covalent Materials Corp | Film thickness measuring method |
-
2012
- 2012-10-26 KR KR1020120119379A patent/KR101241007B1/en active IP Right Grant
-
2013
- 2013-02-20 DE DE112013005159.1T patent/DE112013005159T5/en active Pending
- 2013-02-20 CN CN201380055724.XA patent/CN104769390B/en active Active
- 2013-02-20 WO PCT/KR2013/001312 patent/WO2014065473A1/en active Application Filing
- 2013-02-20 JP JP2015539488A patent/JP6167182B2/en active Active
- 2013-05-14 US US13/893,395 patent/US9644956B2/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| US20140119513A1 (en) | 2014-05-01 |
| CN104769390A (en) | 2015-07-08 |
| DE112013005159T5 (en) | 2015-08-13 |
| JP2015534077A (en) | 2015-11-26 |
| US9644956B2 (en) | 2017-05-09 |
| KR101241007B1 (en) | 2013-03-11 |
| WO2014065473A1 (en) | 2014-05-01 |
| JP6167182B2 (en) | 2017-07-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104769390B (en) | With the method and apparatus of X-ray measurement film thickness | |
| US9746433B2 (en) | X-ray fluorescence spectrometer and X-ray fluorescence analyzing method | |
| Lucarelli et al. | The upgraded external-beam PIXE/PIGE set-up at LABEC for very fast measurements on aerosol samples | |
| Sitko | Quantitative X-ray fluorescence analysis of samples of less than ‘infinite thickness’: difficulties and possibilities | |
| Hodoroaba et al. | Performance of high-resolution SEM/EDX systems equipped with transmission mode (TSEM) for imaging and measurement of size and size distribution of spherical nanoparticles | |
| US20090067573A1 (en) | X-ray measurement of properties of nano-particles | |
| GB2438278A (en) | Energy spectrum modulation and image processing method | |
| JP2003511667A (en) | Identification and verification methods | |
| AU2011203239B2 (en) | Mineral particle material resolving X-ray imaging | |
| TW202124941A (en) | Device and substrate assisted x-ray leakage method for ultrathin film thickness measurement | |
| KR20140118795A (en) | Foreign matter detector | |
| Farquharson et al. | The use of combined trace element XRF and EDXRD data as a histopathology tool using a multivariate analysis approach in characterizing breast tissue | |
| Wobrauschek et al. | X-Ray total reflection fluorescence analysis | |
| JP2009288016A (en) | Fluorescent x-ray analyzer and evaluation system of semiconductor device using it | |
| US20220244159A1 (en) | Water impurity measurements with dynamic light scattering | |
| JP2006313132A (en) | Sample analyzing method and x-ray analyzing system | |
| JP2007078616A (en) | Method and device for measuring thickness of each component layer of thin film comprising a plurality of layers | |
| Nascimento Filho et al. | Limits of detection of a total reflection X-ray fluorescence system with double reflection module | |
| JP6677943B2 (en) | Microspectroscopic data measurement apparatus and method | |
| Loupiac et al. | Neutron imaging and tomography: Applications in food science | |
| Olsansky et al. | High-contrast low-dose proton radiography of thin samples at the Tandetron accelerator | |
| JP2906606B2 (en) | Qualitative analysis of thin film samples | |
| JP2014196925A (en) | Fluorescent x-ray analyzer, and depth direction analysis method used for the same | |
| JP5524663B2 (en) | Fluorescent X-ray film thickness meter and fluorescent X-ray film thickness measuring method | |
| Van Kan et al. | An optimized set-up for total reflection particle induced X-ray emission |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |